A transition-metal coordinated polymer, [Cu(py)2(m-bdc)]n (m-bdc = m-phthalic, py = pyridine) was synthesized using a solvent diffusion method. The crystal structure of the complex was determined by X-ray single crystal diffraction. The result indicates that the polymer is m-phthalic ligand bridged to form a two dimension infinite network structure with a complex crystal data of: monoclinic, space group P 21/c, a =1.0017(5) nm, b=1.1358(6) nm, c=1.7014(7) nm,α=γ=90°,β=114.38(2)°, V=1.7631(15) nm3, Z=15, Dc=1.454 g⋅cm-3. Thermal decomposition mechanism of the complex was investigated by a non-isothermal kinetic method. Iterative iso-conversional methods were applied to calculate the activation energy and the most probable mechanism function was determined by means of the master plots method.The results show that [Cu(py)2(m-bdc)]n begin to decompose at about 170℃ and fully decomposed at 420℃. The decomposition process of [Cu(py)2(m-bdc)]n can be divided into two stages, whose activation energies and the mechanism functions are: Ea = 72.971 kJ⋅mol-1, G(α) = (-ln(-α))0.48 (first stage) and Ea = 179.012 kJ⋅mol-1, G(α)=(-ln(1-α))0.83(second stage), respectively.%采用溶剂扩散法合成了过渡金属配位聚合物：[Cu(py)2(m-bdc)]n (m-bdc =间苯二甲酸，py =吡啶)，根据X-单晶衍射给出配合物的结构，该配合物是由间苯二甲酸根桥连的具有二维无限网状结构的聚合物，为单斜晶系，P 21/c空间群，晶胞参数：a=1.0017(5) nm，b=1.1358(6) nm，c=1.7014(7) nm，α=γ=90°，β=114.38(2)°，V=1.7631(15) nm3，Z=15，Dc=1.454 g⋅cm-3。应用非等温动力学研究技术研究了配合物的热分解机理，采用Ozawa法和KAS法给出了配合物热分解过程的活化能(Ea)，用主曲线法得到了配合物热分解过程的机理函数积分式 G(α)。结果表明：[Cu(py)2(m-bdc)]n在170℃开始分解，420℃分解结束。[Cu(py)2(m-bdc)]n的分解过程分两个阶段完成，两个分解阶段的表观活化能分别为72.971 kJ⋅mol-1，179.012 kJ⋅mol-1；机理函数的积分式分别为：G(α)=(-ln(1-α))0.48(1)、G(α)=(-ln(1-α))0.83(2)。
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